Reaktion #2396362

ord-5a5455e251314c13b390d0213407f274

Reaktionsbedingungen

Temperatur
5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeEvaporation of the solvent
  2. 2
    Sonstigegave a residue, which
  3. 3
    Extraktionwas extracted with ethyl acetate (150 ml)
  4. 4
    WaschenThe extract was washed with water
  5. 5
    Trocknendried over magnesium sulfate
  6. 6
    SonstigeThe solvent was evaporated in vacuo

Vorschrift

To a solution of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (2.024 g) in methylene chloride (60 ml) was added a solution of phenyl chloroformate (1.566 g) in methylene chloride (40 ml) and the mixture was stirred for 4 hours at 5° C. Evaporation of the solvent gave a residue, which was extracted with ethyl acetate (150 ml). The extract was washed with water and dried over magnesium sulfate. The solvent was evaporated in vacuo to give N-(phenoxycarbonylamino)-1,2,3,6-tetrahydropyridine (2.01 g), which was recrystallized from diisopropyl ether to give the desired compound (0.732 g) as colorless needles.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04694004uspto-grants-1987_09